Hydrochloric Acid → Donepezil Hydrochloride

HRID 1454359

반응식

HRID 1454359 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[CH2:14][CH:13]([CH2:15][CH:16]3[CH2:21][CH2:20][N:19]([CH2:22][C:23]4[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=4)[CH2:18][CH2:17]3)[C:11](=[O:12])[C:6]2=[CH:7][C:8]=1[O:9][CH3:10].[ClH:29]>C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[CH2:14][CH:13]([CH2:15][CH:16]3[CH2:17][CH2:18][N:19]([CH2:22][C:23]4[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=4)[CH2:20][CH2:21]3)[C:11](=[O:12])[C:6]2=[CH:7][C:8]=1[O:9][CH3:10].[ClH:29]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 3152Donepezil

생성물 1

HCID 5741Donepezil Hydrochloride수율 95.5%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
9 °C

실험 절차

50 g of donepezil was dissolved by stirring in 315 g of ethanol under heating, followed by adding 15.1 g of concentrated hydrochloric acid thereto at the internal temperature of 30° C. Then, it was cooled and continued stirring while keeping the internal temperature at 30° C. Crystals started precipitating about 30 minutes after the concentrated hydrochloric acid was poured into the mixture. After the precipitation started, the mixture was stirred at the internal temperature of 15° C. for 18 hours and then cooled to the internal temperature of 9° C. The crystals were collected by filtration and dried about 4 hours after the cooling was started, to give 52.32 g of polymorphic crystal (III) of donepezil hydrochloride (yield: 95.5%).

후처리

  1. temperatureunder heating
  2. customat the internal temperature of 30° C
  3. temperatureThen, it was cooled
  4. customat 30° C
  5. customCrystals started precipitating about 30 minutes after the concentrated hydrochloric acid
  6. additionwas poured into the mixture
  7. customAfter the precipitation
  8. stirringthe mixture was stirred at the internal temperature of 15° C. for 18 hours
  9. filtrationThe crystals were collected by filtration
  10. customdried about 4 hours after the cooling

출처 및 근거

ORD 기록
ord-c48548638fda44cea3f27cca165efcd3
출처 데이터셋
uspto-grants-2009_01
특허 번호
US07479563B2

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